Jean chaeles octave chemist



UNITED STATES PATENT OFFICEZIQ JEAN CHARLES OOTAVE OI-IEMIN, OF PARIS,FRANCE.

PROCESS OF PREPARING OZOCERITE AND OTHER SOLID HYDROCARBONS.

SPECIFICATION forming part of Letters Patent No. 297,766, dated April29, 1884.

Application filed July 28, 1883. (No specimens.)

.Z 0 aZZ whom it may concern.-

Be it known that I, JEAN CHARLES Ocrnvn OHEMIN, a citizen of the FrenchRepublic, residing at Paris, France, have invented certain Improvementsin the Process of Preparing Ozocerite and other Solid Hydrocarbons, ofwhich the following is a specification.

My object is to purify and bleach ozocerite, paraffine, and other solidor semi-solid hydrocarbons in order to fit them for waxing floors,furniture, &c., and for use in the arts, as in the manufacture ofharness, &c.

I11 carrying out my invention where ozocerite, for example, is to betreated, vI employ the process I will now describe, which I divide intosteps, as follows:

First. Ozocerite in the raw or crude stat has a marked tendency tobecome darker when heated above its point of fusion. To facilitate thebleaching of this substance by my process, I melt the crude material inwater heated to and maintained'at a temperature of 70 centigrade. Theearthyand solid impurities contained in it fall to the bottom of themeltingvessel. On decanting and cooling, I thus obtain a product muchless colored than the commercial product and well suited to undergo thefurther operations of the process.

Second. The ozocerite, prepared as above described, is placed in aretort to which direct .heat may be applied, and in which is' arrangedsuitable apparatus for injecting superheated steam. NV hen the substanceis melted, I add flowers of sulphur in the proportion of five to fifteenper centum, the proportion varying somewhat above and below theselimits, according to the nature and character of the 020- cerite. Theheating of the retort and the application of the superheated steam toits contents may be efiected in any of the ways well known instearine-works. The distillation effected is not fractional. Thedistillate is yellow, homogeneous, and without fluorescence ordichroism. It crystallizes by slow cooling, and is in excellentcondition to be submitted to the after steps of the process. Theimmediate yield is from ninety-two to ninety-five per centum of thematerial submitted to distillation.

Third, For this step in the process I may employ either of the two modesfollowingz m.)

. stirred vigorously, and when the digestion is The distillate abovedescribed is run into molds, such as are employed in stearine-works. Thecakes obtained are submitted'to heat and pressure, the platens of thepress being main- .5 5

tained at a temperature of from 35 to This pressure expels the majorpart of the oils and hydrocarbons fusible at low temperature. (1).) Thedistillate reduced to powder by any known means-as by insufilation, forexample-is introduced into a hydro extractor, which is maintained at atemperature of from 40 to 50 centigrade. Into this extractor waterheated to from 45 to is introduced as a spray. This spray facilitatesthe extraction of the oils and hydrocarbons fusible at low temperatures.The above operation may be eifected at the ordinary temperature bysubstituting for the hot water amylic alcohol'or any otherv knownsolvent of oils and liquid bydrocarbons. Fourth. The product obtained byeither 0 the steps a and b is fused in a hot-water bath (bain-marie) ata temperature of to Amylic alcohol to the amount of about twenty turevigorously stirred to insure a thorough mixture, and the substance isrun into molds and allowed to cool. These solid blocks are thensubmitted to pressure in a-hydraulic press, and the cakes from the pressare melted and allowed to digest during about four hours with animalcharcoal; During all this time the mixture of animal black and ozoceriteis 5 finished the substance is filtered through animal charcoal. Theproduct thus obtained is, when cooled, perfectly white, hard, andsonorous, and comprises from seventy nine to eighty-one per centum ofthe product submitted to distillation. The liquids yielded by this lastoperation, as well as those which result from the treatment with amylicalcohol or other solvents, are distilled to recover said alcohol orother solvents, which may be used again. The residue is mixed with newcharges of the material, to be subsequently treated, and thus all wasteis practically avoided.

To render the operationsstill easier, I have found-advantage in mixingthe ozocerites with 100 theresidues from Pennsylvania petroleum ornaphtha. The proportions will vary somewhat, according to thecircumstances; but a medium proportion is from seventy to eighty percentum of ozoeerite to from twenty to thirty per centum of the petroleumresidue. 5 The yield in this case will be somewhat modified from thefigures given above.

My above-described process is adapted not only to the treatment ofozoeerite, but to all solid or semi-liquid hydrocarbons-as, for example,residues of petroleum and naphtha, tars of all kinds, distillates frombituminous schists, &c.,which substances may be purified and bleachedthereby. In the first step of my process when applied to many of thesesubstances, it is well to employ filter-presses provided with thewell-known Mirandaz apparatus, which introduces the substance into thefilters.

The action of the sulphur in my process is somewhat difficult toexplain. I have established the fact experimentally that it acts mostpowerfully as a dceolorizing agent when the ozocerite is melted at itslowest temperature. Therefore I have indicated the fusion with abain-marie at a temperature of 70 eentigrade. In all the reactions thesulphur acts as much by its presence as by reason of the combinations towhich it gives rise. Vhen used with the molten ozocerite, it isnecessary to mix it uniformly through the molten mass. At the beginningof the distillation the gaseous products expelled by the current ofsuperheated steam contain a notable proportion of sulphureted hydrogen,and when the disengage ment of this gas ceases, it is replaced bypolysnlphurets, likewise gaseous, and having characteristic odors. Ofthese I have not been able yet to determine the exact composition. Theproduct of the distillation contains only traces of sulphur,or perhapssulphurets. It is known that hydrocarbons dissolve a certain proportionof this metalloid. XVhen flower of sulphur is mixed with moltenozocerite, (without distillation,) it passes through the mass by brownto an ocher-yellow. The higher the reason of its gravity, and falls tothe lowertemperature at which the ozoeerite has been fused the lesspronounced will be the decolorizing effect of the sulphur.

I am aware that amylic alcohol has been employed in treatinghydrocarbons, and I make no claim to this.

Having thus described my invention, I claim 1. The herein-describedmethod of treating or preparing ozoeerite and other similarhydroearbons,which consists in first removing the earthy insolubleimpurities by the means substantially as described, then heating thethus purified substance in a retort in connection with sulphur in aboutthe proportions specified, and submitting the same to the action ofsuperheated steam in the retort until it distills over, substantially asset forth.

2. The herein-described method of treating or preparing ozocerite andother similar 11ydrocarbons, which consists in first removing the earthyinsoluble impurities, substantially as described, then distilling thethus purified hydrocarbon in combination with flowers of sulphur,substantially as specified, and then removing the oils and lighterhydrocarbons in the manner described, substantially as and for thepurposes set forth.

3. The herein-described method of purifying and bleaching ozocerite andsimilar hydrocarbons, which consists in first removing the earthyinsoluble impurities, as herein set forth second, distilling the thuspurified 11ydroearbon mixed with flowers of sulphur in about theproportions specified; third, removing the oils and lighter hydrocarbonsby heat and pressure, or the specified equivalent of the same; fourth,fusing in a bath with amylic alcohol, cooling and pressing, digestingwith animal charcoal while in a molten state, and finally filteringthrough animal charcoal, substantially as set forth.

In witness whereof I have hereunto signed my name in the presence of twosubscribing witnesses.

JEAN CHARLES OCTAVE CllEZlllN.

Vitnesses:

EDWARD 1?. MAcLnAN, AMANI) Rrr'rER.

